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Following the introduction of lead-free frangible ammunition in United States Air Force small arms firing ranges, Combat Arms instructors have routinely reported experiencing adverse health symptoms during live fire training exercises, including sore throat, cough, and headache. Previous studies have found that these symptoms occur despite occupational exposure limits not being exceeded. To better characterize the potential source and mechanisms for health symptoms, a comprehensive characterization of the physicochemical properties of gases and aerosols emitted during the firing of the M9 pistol and M4 rifle using lead-free frangible ammunition was completed. Weapons were fired within a sealed chamber using a remote firing mechanism. A suite of direct-reading instruments and collection-based analytical methods were used to determine the composition of the emissions. Emissions were dominated by carbon monoxide and ultrafine particles. Other prevalent gases included carbon dioxide, ammonia, formaldehyde, hydrogen cyanide, and nitric oxide when measured using Fourier-transform infrared spectroscopy. An electrical, low-pressure impactor showed that, on average, the count median diameter immediately after firing was 36 ± 4 nm (n = 10 rounds) and 32 ± 3 nm (n = 14 rounds) for the M9 pistol and M4 rifle, respectively. Analytical methods were used to determine that emitted particles were primarily composed of soot, copper, and potassium, with trace amounts of calcium, silicon, sodium, sulfur, and zinc. Results from this research confirm prior work and expand upon the characterization of emissions generated from firing lead-free frangible ammunition. By employing multiple methods to measure and analyze data we were able to quantify both total and respirable particle fractions and determine particle morphology and composition. Characterization of the emissions provides insight into potential exposure risks that may lead to the development of adverse health symptoms allowing for the development of strategies for risk mitigation.